Journal of Chromatography A, 1160 (2007) 81–89
Determination of essential oil components of Artemisia haussknechtii
Boiss. using simultaneous hydrodistillation-static headspace liquid
phase microextraction-gas chromatography mass spectrometry
M. Jalali Heravi
a,∗
, H. Sereshti
b
a
Department of Chemistry, Sharif University of Technology, P.O. Box 11365-9516, Tehran, Iran
b
Department of Chemistry, Faculty of Sciences, University of Tehran, Tehran, Iran
Received 24 November 2006; received in revised form 7 April 2007; accepted 15 May 2007
Available online 7 June 2007
Abstract
A novel method for extraction and analysis of volatile compounds of Artemisia haussknechtii Boiss., using simultaneous hydro-distillation and
static headspace liquid microextraction followed by gas chromatography–mass spectrometry (SHD-SHLPME-GCMS) is developed. SHLPME
parameters including nature of extracting solvent, headspace volume and design, extraction time, sample weight and microdrop volume were
optimized. Comparison of hydro-distillation gas chromatography–mass spectrometry and HD-SHLPME-GCMS showed that the latter method
is fast, simple, inexpensive and effective for the analysis of volatile compounds of aromatic plants. By using this method, 56 compounds were
extracted and identified for Artemisia haussknechtii Boiss. The main constituents of its essential oil that were extracted by HD-SHLPME method,
include camphor (41.01%), 1,8-cineole (32.35%), cis-davanone (3.68%), 4-terpineol (2.99%), linalool (2.84%), beta-fenchyl alcohol (2.72%), and
borneol (2.58%).
© 2007 Elsevier B.V. All rights reserved.
Keywords: Hydrodistillation (HD); Hydrodistillation-static headspace liquid phase microextraction (SHD-SHLPME); Artemisia haussknechtii Boiss.; Essential oil;
Single drop microextraction; Gas chromatography–mass spectrometry (GC–MS)
1. Introduction
As the sophisticated analytical instruments are not capable
of handling sample matrices directly, a sample preparation step
is required. Sample preparation is a critical step in an analytical
procedure. The main aim of sample preparation is to transfer the
analyte into a form that is prepurified, concentrated, and compat-
ible with the analytical system [1]. Main advantages of sample
preparation procedures such as solvent microextraction (SME)
and headspace sampling (HSS) [2] are their speed and small
volume of solvents required for their performances. Single-drop
microextraction that is the advanced type of this approach is
a simple, inexpensive, fast, effective and virtually solvent-free
sample pretreatment technique. The major idea behind this has
been to facilitate automation, to speed up extractions, and to
reduce the consumption of organic solvents. Generally, there are
two different modes of liquid phase microextraction (LPME):
∗
Corresponding author. Tel.: +98 21 66005718; fax: +98 21 66012983.
E-mail address: jalali@sharif.edu (M. Jalali Heravi).
static LPME consisted of a microdrop suspended at the tip of a
microsyringe needle and dynamic LPME, in which the microsy-
ringe is used as a separatory funnel and featured the repeated
movement of the syringe plunger [3–9]. Headspace microex-
traction (HSME) is a combination of HSS and SME, and has the
high capabilities of them. It is a novel method that can be used
for the sample preparation in chromatographic analysis [10–12].
HSME is shown to be an efficient preconcentration method for
extraction of volatile compounds from aqueous sample solu-
tions [13]. Direct headspace analysis of volatile compounds in
aqueous or other matrices is utilized extensively for years as a
mean of directly determining volatile compounds without inter-
ference from the sample matrix. In such determinations, the
headspace is typically sampled directly with a microsyringe,
therefore, it is applicable only to extremely volatile compounds
[14].
Essential oils (EOs, also called volatile or ethereal oils) are
aromatic oily liquids obtained from plant materials. The greatest
use of EOs is in food (as flavorings), perfumes and pharma-
ceuticals (for their functional properties) [15]. To achieve the
0021-9673/$ – see front matter © 2007 Elsevier B.V. All rights reserved.
doi:10.1016/j.chroma.2007.05.096